CN109876786A - A kind of method of low melting point solid peracid regenerating waste active carbon - Google Patents

A kind of method of low melting point solid peracid regenerating waste active carbon Download PDF

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Publication number
CN109876786A
CN109876786A CN201910282358.0A CN201910282358A CN109876786A CN 109876786 A CN109876786 A CN 109876786A CN 201910282358 A CN201910282358 A CN 201910282358A CN 109876786 A CN109876786 A CN 109876786A
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active carbon
acid
solid peracid
melting point
peracid
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CN201910282358.0A
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CN109876786B (en
Inventor
林冠烽
蔡政汉
杨旋
黄彪
王琼
李涛
荣成
陈燕丹
陈学榕
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Fujian Xinsen Carbon Co ltd
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Fujian Agriculture and Forestry University
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Abstract

The invention discloses a kind of methods of low melting point solid peracid regenerating waste active carbon, belong to active carbon regenerating technology field.The present invention is reacted certain time at a constant temperature, is cooled down later by melting solid peracid and discarded active carbon, and hot water is added, filters while hot, and is washed with hot water to pH5-7, dry to get regenerated carbon.Using solid peracid unique performance in the molten state, there is very strong degradation catalytic action to organic adsorbate, adsorbate quickly can be degraded into small molecule, and it is carried out catalysis and changes chemical property, it is dissolved in it in acid, realizes the removing of adsorbate, reach regenerated purpose.Preparation method of the invention is easy to operate, and the reaction time is short, high production efficiency, realizes the effective regeneration of active carbon, and solid peracid used is easily recycled, and can be recycled, and no waste liquid generates, low in cost, environmentally protective.

Description

A kind of method of low melting point solid peracid regenerating waste active carbon
Technical field
The invention belongs to regenerating active carbon fields, and in particular to a kind of side of low melting point solid peracid regenerating waste active carbon Method.
Background technique
Active carbon is a kind of environmentally friendly adsorbent, and maximum obstacle is higher cost in use process, and That there are regeneration energy consumptions after adsorption saturation is higher, yield is lower, easily causes secondary pollution problems.Therefore, new regeneration is found Method reaches active carbon and recycles to reduce energy consumption, it appears and it is extremely urgent, the hot spot of research tackling key problem will be become.The present invention Low melting point solid peracid is applied to the regeneration of active carbon, this method is easy to operate, and the reaction time is short, and high production efficiency realizes The effective regeneration of active carbon, and solid peracid used is easily recycled, and can be recycled, and no waste liquid generates, low in cost, green ring It protects.Therefore, this method will promote regenerating active carbon process economics feasible, to development low-carbon economy, energy-saving and emission-reduction, protection be promoted to give birth to State environment and sustainable development have great strategic significance.
Regenerating active carbon refers to under the premise of not destroying active carbon original structure, either physically or chemically adsorbing Adsorbate in active carbon hole is removed, and is restored its absorption property, is achieved the purpose that reuse.Using which kind of method It carries out regenerating active carbon and depends primarily on the type of active carbon and the property of adsorbent, while regenerative operation will guarantee absorption The active carbon hole of effect should not lose too much.Currently, the regeneration method of active carbon used both at home and abroad mainly has: hot recycling method, Bio-regeneration method, wet air regeneration method, solvent extraction method of reproduction, electrochemical regeneration method, microwave irradiation method of reproduction, ultrasonic wave are again It thinks of a way, supercritical CO2Extract the methods of method of reproduction, ozone oxidation method of reproduction and Photocatalytic Regeneration method.
Low melting point solid peracid in the molten state, has its unique performance.Melting acid has very organic adsorbate Strong degradation catalytic action, quickly can be degraded into small molecule for partial adsorbates matter, and is carried out catalysis and change chemical property, make It is dissolved in acid, realizes the removing of adsorbate, reaches regenerated purpose.Such as the craboraffin for adsorption saturation, melting Disaccharides can be degraded into monosaccharide by acid, by monosaccharide hydroxyl by catalysis carboxyl grafting, be easily more soluble among acid, reached regeneration mesh 's.Meanwhile the solid peracid of molten condition, it can be considered a kind of solvent, to the adsorbate that can not be degraded, make with certain dissolution With further increasing the regeneration effect of active carbon.
Summary of the invention
It is an object of the invention to be directed to the deficiency of existing active carbon regenerating technology, a kind of low melting point solid peracid is provided again The method of raw discarded active carbon.This method is easy to operate, and the reaction time is short, high production efficiency, realize active carbon effectively again It is raw;Its solid peracid used is easily recycled, and can be recycled, and no waste liquid generates, low in cost, environmentally protective.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of method of low melting point solid peracid regenerating waste active carbon, comprising the following steps:
(1) after solid peracid being heated to molten condition, discarded active carbon is added, isothermal reaction certain time obtains discarded activity Charcoal-melting solid-state acid blend;
(2) it is cooled to 60-90 DEG C to the resulting discarded active carbon of step (1)-melting solid-state acid blend, hot water is added, while hot Filtering, and continuing to be washed with hot water to pH value is 5-7, obtains active carbon.
(3) active carbon obtained in step (2) is dried to get regenerated carbon, and the filtrate of step (2) is steamed Hair crystallization, recycles solid peracid.
Solid peracid described in above-mentioned steps (1) include succinic acid, oxalic acid, glutaric acid, adipic acid, azelaic acid, metaphosphoric acid, Any one in citric acid, gluconic acid.Low melting point solid peracid and its fusing point are shown in Table 1.
1 solid peracid of table and its fusing point
Discarded active carbon described in above-mentioned steps (1) is the active carbon adsorbed after organic substance;Discarded active carbon and solid peracid Mass ratio be 1:3-1:20.
Isothermal reaction certain time described in above-mentioned steps (1), reaction temperature are 70-190 DEG C, and the reaction time is 5min-4h, processing mode are magnetic agitation.
The mass ratio of addition hot water and solid peracid described in above-mentioned steps (2) is 1:5-1:20.
The temperature that hot water is added described in above-mentioned steps (2) is 50-90 DEG C.
The present invention has the advantages that
(1) low melting point solid peracid unique performance in the molten state is utilized, there is very strong degradation to urge organic adsorbate Change effect, quickly can be degraded into small molecule for adsorbate, and is carried out catalysis and change chemical property, be dissolved in it in acid, real The removing of existing adsorbate, reaches regenerated purpose.Such as adsorbate in craboraffin, disaccharides can be degraded by melting acid Monosaccharide is easily more soluble among melting acid by monosaccharide hydroxyl by catalysis carboxyl grafting, reaches regenerated purpose.Meanwhile it is molten The solid peracid for melting state can be considered a kind of solvent, to the adsorbate that can not be degraded, has certain dissolution, further mentions Its high regeneration effect.
(2) operation of the present invention is simple, and the reaction time is short, and low energy consumption, low in cost, high-efficient.
(2) present invention has effectively restored adsorption capacity and specific surface area, realizes the highly efficient regeneration of discarded active carbon.
(3) solid peracid used in the present invention is non-hazardous to environment, and easily recycles, and can reuse, environmentally protective.
Specific embodiment
The present invention is further illustrated by the following examples, but protection scope of the present invention is not limited to following reality Example.
Embodiment 1
By the succinic acid of 150g technical grade, be heated to 185 DEG C melt succinic acid completely after, 10g is added and discards active carbon, 185 DEG C constant temperature is handled 2 hours, obtains discarded active carbon-melting solid-state acid blend;Then active carbon to be discarded-melting solid-state acid-mixed It closes object and is cooled to 90 DEG C, 50 DEG C of hot water of 30mL are added in said mixture, are filtered while hot, washing to pH is 5-7, drying.Filter Liquid is through evaporative crystallization recycling succinic acid to recycle.
The specific surface area that active carbon is discarded in this example is 636m2/ g, iodine sorption value 567mg/g, what is obtained lives again Property charcoal specific surface area be 921m2/ g, iodine number 832mg/g, yield 94%.
Embodiment 2
After 105 DEG C in the oxalic acid of 200g technical grade, will be heated to melting oxalic acid completely, 10g is added and discards active carbon, 105 DEG C Constant temperature is handled 2 hours, obtains discarded active carbon-melting solid-state acid blend.Active carbon to be discarded-melting solid-state acid blend drop 60 DEG C of hot water hot water of 10mL are added in said mixture, filter while hot to 60 DEG C by temperature, and washing to pH is 5-7, drying.Filtrate Through evaporative crystallization recycling oxalic acid to recycle.
The specific surface area that active carbon is discarded in this example is 636m2/ g, iodine sorption value 567mg/g, obtains regeneration activity The specific surface area of charcoal is 1240m2/ g, iodine number 986mg/g, yield 92%.
Embodiment 3
150g technical grade glutaric acid is heated to 100 DEG C, after melting glutaric acid completely, the discarded active carbon of addition 15g, 100 DEG C Isothermal reaction 2 hours, obtain discarded active carbon-melting solid-state acid blend;Active carbon to be discarded-melting solid-state acid blend drop Temperature is added 80 DEG C of hot water of 20mL, filters while hot to 80 DEG C, and washing to pH is 5-7, drying.Filtrate recycles oxalic acid through evaporative crystallization To recycle.
The specific surface area that active carbon is discarded in this example is 636m2/ g, iodine sorption value 567mg/g, obtains regeneration activity The specific surface area of charcoal is 1130m2/ g, iodine number 955mg/g, yield 92%.
Embodiment 4
50g citric acid is heated to 153 DEG C, after melting citric acid completely, 10g is added and discards active carbon, 153 DEG C of constant temperature processing 3 hours, obtain discarded active carbon-melting solid-state acid blend;Active carbon to be discarded-melting solid-state acid blend is cooled to 90 DEG C, 90 DEG C of hot water of 10mL are added in said mixture, are filtered while hot, washing to pH is 5-7, drying.Filtrate is through evaporative crystallization Citric acid is recycled to recycle.
The specific surface area that active carbon is discarded in this example is 636m2/ g, iodine sorption value 567mg/g, what is obtained lives again Property charcoal specific surface area be 1024m2/ g, iodine number 931mg/g, yield 94%.
Embodiment 5
15g metaphosphoric acid is heated to 74 DEG C, after melting metaphosphoric acid completely, 5g is added and discards active carbon, 74 DEG C of constant temperature processing 4 are small When, obtain discarded active carbon-melting solid-state acid blend;Active carbon to be discarded-melting solid-state acid blend is cooled to 60 DEG C, will 50 DEG C of hot water of 3mL are added in said mixture, filter while hot, and washing to pH is 5-7, drying.Filtrate is recycled inclined through evaporative crystallization Phosphoric acid is to recycle.
The specific surface area that active carbon is discarded in this example is 636m2/ g, iodine sorption value 567mg/g, what is obtained lives again Property charcoal specific surface area be 986m2/ g, iodine number are 892 mg/g, yield 96%.
Embodiment 6
50g gluconic acid is heated to 131 DEG C, after melting gluconic acid completely, 5g is added and discards active carbon, 131 DEG C of constant temperature 5min is handled, discarded active carbon-melting solid-state acid blend is obtained;Active carbon to be discarded-melting solid-state acid blend is cooled to 90 DEG C, 70 DEG C of hot water of 10mL are added in said mixture, are filtered while hot, washing to pH is 5-7, drying.Filtrate is tied through evaporation Crystalline substance recycling gluconic acid is to recycle.
The specific surface area that active carbon is discarded in this example is 636m2/ g, iodine sorption value 567mg/g, what is obtained lives again Property charcoal specific surface area be 968m2/ g, iodine number are 812 mg/g, yield 97%.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with Modification, is all covered by the present invention.

Claims (7)

1. a kind of method of low melting point solid peracid regenerating waste active carbon, which comprises the following steps:
(1) after solid peracid being heated to molten condition, discarded active carbon is added, isothermal reaction certain time obtains discarded activity Charcoal-melting solid-state acid blend;
(2) it is cooled to 60-90 DEG C to the resulting discarded active carbon of step (1)-melting solid-state acid blend, hot water is added, while hot Filtering, and continuing to be washed with hot water to pH value is 5-7, obtains active carbon;
(3) active carbon obtained in step (2) is dried to get regenerated carbon, and the filtrate of step (2) is evaporated and is tied Crystalline substance recycles solid peracid.
2. a kind of method of low melting point solid peracid regenerating waste active carbon according to claim 1, it is characterised in that: described Solid peracid in step (1) includes succinic acid, oxalic acid, glutaric acid, adipic acid, azelaic acid, metaphosphoric acid, citric acid, gluconic acid In any one.
3. a kind of method of low melting point solid peracid regenerating waste active carbon according to claim 1, it is characterised in that: described Discarded active carbon in step (1) is the active carbon adsorbed after organic substance, and the mass ratio for discarding active carbon and solid peracid is 1: 3-1:20。
4. a kind of method of low melting point solid peracid regenerating waste active carbon according to claim 1, it is characterised in that: described Isothermal reaction certain time in step (1), reaction temperature are 70-190 DEG C, reaction time 5min-4h.
5. a kind of method of low melting point solid peracid regenerating waste active carbon according to claim 1, it is characterised in that: described The mass ratio that hot water and solid peracid are added in step (2) is 1:5-1:20.
6. a kind of method of low melting point solid peracid regenerating waste active carbon according to claim 1, it is characterised in that: described The temperature that hot water is added in step (2) is 50-90 DEG C.
7. the regenerated carbon obtained such as claim 1-6 the method.
CN201910282358.0A 2019-04-09 2019-04-09 Method for regenerating waste activated carbon by using low-melting-point solid acid Active CN109876786B (en)

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Effective date of registration: 20221109

Address after: Lianfu Road, Chengjiao Industrial Park, Shaowu City, Nanping City, Fujian Province, 354000

Patentee after: FUJIAN XINSEN CARBON Co.,Ltd.

Address before: No. 15, Cangshan District, Fujian, Fuzhou, Fujian

Patentee before: FUJIAN AGRICULTURE AND FORESTRY University